| 63 | 0 | 65 |
| 下载次数 | 被引频次 | 阅读次数 |
建立了一种液相色谱-串联质谱法(LC-MS/MS)，可同时对血液中25种常见有机磷农药(OPs)进行定性定量检测，旨在为公安机关侦办中毒案件及非正常死亡案件提供有力技术支撑。以V(甲醇)∶V(乙腈)=1∶1为提取溶剂，并用V(血液样品)∶V(提取剂)=1∶5混合溶液进行蛋白沉淀，涡旋5 min，以8000 r/min离心5 min，获得的上清液经0.22μm尼龙微孔滤膜过滤后采用Shim-pack GIST C18-AQ色谱柱在梯度淋洗条件下进行分离。质谱分析在电喷雾离子源正离子模式(ESI+)下进行，多反应监测(MRM)模式检测，基质外标法进行定量分析。方法学验证结果表明，血液中25种OPs峰形良好，在10～250 ng/m L质量浓度范围内具有良好的线性响应，线性关系均大于0.992，检出限为0.02～2.53 ng/m L，定量限为0.05～8.33 ng/m L。空白加标样品在20、100、200 ng/m L这3个加标水平时，25种目标物在血液中提取回收率为67.57%～129.35%，相对标准偏差为0.37%～12.85%。该方法前处理操作简单，具有较高的准确性和可靠性，可同时对血液中25种OPs进行定性、定量分析，为实际案件侦办中人体血液样品中常见OPs成分的检测提供可靠的科学依据。
Abstract：A liquid chromatography-tandem mass spectrometry( LC-MS/MS) method was established for the simultaneous qualitative and quantitative detection of 25 common organophosphorus pesticides( OPs) in blood,aiming to provide robust technical support for public security authorities in investigating poisoning cases and unnatural death cases. A mixed solution of V( methanol) ∶ V( acetonitrile) = 1 ∶1 was used as the extraction solvent,V( blood samples) ∶ V( the extractant) = 1 ∶5 mixed solution was used as for protein precipitation,vortexed for 5 min,and centrifuged at 8000 r/min for 5 min. The supernatant obtained was filtered through a 0. 22 μm nylon microporous membrane and then separated on a Shim-pack GIST C18AQ column under gradient elution conditions. Mass spectrometric analysis was performed in positive electrospray ionization mode( ESI+) with multiple reaction monitoring( MRM),and matrix matched external standard method was used for quantitative analysis. Methodological validation demonstrated that the 25 OPs in blood had good peak shapes and good linearity over the concentration range of 10 ～ 250 ng/m L,with all correlation coefficients exceeding 0. 992. The limits of detection were 0. 02 ～ 2. 53 ng/m L,and the limits of quantification were 0. 05 ～ 8. 33 ng/m L.For blank spiked samples at three spiking levels of 20,100,and 200 ng/m L,the extraction recoveries of the 25 target analytes in blood ranged from 67. 57% to 129. 35%,with relative standard deviations( RSDs) of0. 37% ～ 12. 85%.This method features simple pretreatment,high accuracy,and good reliability,enabling simultaneous qualitative and quantitative analysis of 25 OPs in blood.It provided a reliable scientific basis for the detection of common OPs components in human blood samples in practical case investigations.
[1]Sarath C C,Thomas S. Organic Farming:New Advances Towards Sustainable Agricultural Systems. Berlin:Springer,2019.
[2]Kaur R,Mavi G K,Raghav S,Khan I.Int.J.Curr.Microbiol.App.Sci,2019,8(3):1889-1897.
[3]He X L,Nie Y,Wang N,Xia H N,Liu J Y,Lu Y X,He M.Environ.Ecol.,2021,3(10):38-43．何小玲，聂艳，王念，夏华南，刘嘉宇，卢雨萱，贺美．环境生态学，2021,3(10):38-43.
[4]Chen X Q.Guangxi Med.J.,2004,6:773-775．陈晓琴．广西医学，2004,6:773-775.
[5]Li Z.Xin Nongye,2026,4:26-27．李喆．新农业，2026,4:26-27.
[6]Kim H S,Kim J,Suh J H,Han S B. Arch. Pharm. Res.,2014,37(10):1317-1324.
[7]Rosano T G,Ohouo P Y,Leque J J,Freeto S M,Wood M.J.Anal.Toxicol.,2016,40(8):628-638.
[8]Klepacki J,Davari B,Boulet M,Lizarraga R,Christians U.Ther.Drug Monit.,2017,39(5):565-574.
[9]Peng C,Xiong Y,Wang N.J.Agric.Catastr.,2026,16(3):37-39．彭超，熊燕，王娜．农业灾害研究，2026,16(3):37-39.
[10]Fu L X,Zhuo X C,Xu F,Wang B J,Wu Y Z,Xu N L,Chen F,Tao J,Shao P Y. Chin. J. Forensic Med.,2022,37(6):565-570．富利祥，卓晓聪，徐峰，王斌杰，吴元钊，徐念来，陈峰，陶俊，邵朋阳．中国法医学杂志，2022,37(6):565-570.
[11]Chen M,Yin Q,Deng Q,Liu Q,Zhang Y R,Yang X F.Chin.J.Anal.Lab.,2024,43(1):70-78．陈敏，尹全，邓强，刘茜，张义蓉，杨晓凤．分析试验室，2024,43(1):70-78.
[12]Liu F,Li T D,Xie Y X. Occupation Heal.,2016,32(24):3345-3348．刘奋，李添娣，谢玉璇．职业与健康，2016,32(24):3345-3348.
[13]Cheng Z,Zhang R,Liu W H,Wang J H,Wang M L.Chin.J.Chromatogr.,2014,32(1):57-68．程志，张蓉，刘韦华，王金花，王明林．色谱，2014,32(1):57-68.
[14]Li C M,Hu X Y,Fan C L,Zhang B L,Peng T,Chang Q Y,Pang G F,Wang W W. J. Instrumental Anal.,2017,36(4):431-448．李春苗，胡雪艳，范春林，张博伦，彭涛，常巧英，庞国芳，王雯雯．分析测试学报，2017,36(4):431-448.
[15]Jouybari T A,Jouybari H A,Ataee M,Hosseini F,Pasdar Y,Fattahi N. Environ. Sci. Pollut. Res.,2024,31:55812-55821.
[16]Han M,Hou X,Qiu S T,Wang Y H.J.Food Saf.Qual.,2019,10(10):3065-3077．韩梅，侯雪，邱世婷，王悦涵．食品安全质量检测学报，2019,10(10):3065-3077.
[17]Zeng Q X,Huang M X,Liu Z B,Gao Y F,Wang G H,Chen X C.Chem.Reag.,2023,45(11):104-110．曾秋霞，黄敏兴，刘泽槟，高裕锋，王桂华，陈晓初．化学试剂，2023,45(11):104-110.
[18]Peng F,Tan Y Y,Zhang S S,Yu X F,Chen H X.J.Hubei Univ.Nat.Sci.,2021,43(2):109-115．彭帆，谭雨嫣，张珊珊，余小芳，陈怀侠．湖北大学学报(自然科学版)，2021,43(2):109-115.
[19]Du Q Y,Zhang Y F,Wang J F,Wang L,Chang J,Dong L P,Wu X J,Liu B J. J. Instrumental Anal.,2020,39(4):485-491．杜秋瑶，张云峰，王继芬，王璐，常靖，董林沛，吴小军，刘冰洁．分析测试学报，2020,39(4):485-491.
[20]Bai L W,Wang R H,Yu Z S,Zhong S H,Yu Z.Chem.Res.Appl.,2020,32(1):150-156．白利文，王瑞花，于忠山，钟世豪，于哲．化学研究与应用，2020,32(1):150-156.
[21]Li Z M,Ma C G,Li Y H,Gan Y L,Yang Z L.Chem.Reag.,2026,48(2):58-65．李增明，马春光，李玉环，甘瑛琳，杨增亮．化学试剂，2026,48(2):58-65.
[22]Zhu L H,Wu Q Y,Chen W K,Liu D H,Chen X,Mou G Z.Chem.Reag.,2025,47(7):102-107．朱良辉，吴倩颖，陈伟康，刘德鸿，陈希，缪贵忠．化学试剂，2025,47(7):102-107.
[23]Yang S Y,He H Y,Jiang L W,Lv J X,Teng A X.J.Instrum.Anal.,2025,44(4):583-592．杨思瑶，何洪源，蒋力维，吕建霞，滕傲雪．分析测试学报，2025,44(4):583-592.
[24]Yang Z,Jiang L W,Yang S Y,Wu Y D,Lv J X.Chin.J.Chromatogr.,2024,42(10):943-953．杨哲，蒋力维，杨思瑶，吴一荻，吕建霞．色谱，2024,42(10):943-953.
基本信息:
DOI：10.13822/j.cnki.hxsj.2026.0162
中图分类号:R446.11;O657.63
引用信息:
[1]万耔莘,蒋力维,闫昕,等.液相色谱-串联质谱法同时检测血液中25种有机磷农药[J].化学试剂,2026,48(08):57-63.DOI:10.13822/j.cnki.hxsj.2026.0162.
基金信息:
北京市科技计划项目(Z221100005222006)
2026-07-02
2026
2026-07-22
2026-07-29
2026
1
2026-07-28
2026-07-28
2026-07-28